CN116120932A - Layered double perovskite fluorescent material and preparation method thereof - Google Patents
Layered double perovskite fluorescent material and preparation method thereof Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052761 rare earth metal Inorganic materials 0.000 description 3
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- PNKUSGQVOMIXLU-UHFFFAOYSA-N Formamidine Chemical compound NC=N PNKUSGQVOMIXLU-UHFFFAOYSA-N 0.000 description 2
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- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
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- 229910052745 lead Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/7428—Halogenides
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Abstract
The invention discloses a layered double perovskite fluorescent material, which is prepared from the following materials in percentage by mole: csX:50 to 60mol percent; mnX 2 ：10～20mol％；BiX 3 :20 to 30mol%; x is one or more of Cl, br, I, F elements; mixing the raw materials, placing into an agate mortar, dripping deionized water, grinding, drying, grinding into powder, placing into a heating furnace, heating, preserving heat, and cooling to room temperature. The method adopts a solid phase method, the raw materials are cheap and easy to obtain, no strong acid solvent polluting the environment is used, no harmful waste is generated, the reaction condition is mild, the sample does not need further purification, and the method is easy to operate, low in cost and environment-friendly; the product of the invention has good stability and good quantum efficiency, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of double perovskite photoluminescence fluorescence, and particularly relates to a layered double perovskite fluorescent material and a preparation method thereof.
Background
As a new generation of luminescent materials, metal halides have attracted increasing attention in many research fields of photovoltaics, photodetection, illumination, display, scintillators, and the like, due to their unique photoelectric properties, including high quantum yield, large absorption coefficient, long carrier diffusion distance, tunable band gap. Unfortunately, conventional metal halidesPerovskite (general formula ABX) 3 Where A is Methylamine (MA), formamidine (FA) or Cs, B is Pb or Sn, etc., and X is Cl, br or I) shows poor stability to light, heat, water, etc., due to the toxicity of lead, which seriously hinders their commercial applications.
As an alternative, lead-free halide double perovskite and its derivative structure overcomes the drawbacks of lead-containing metal halide perovskite, achieves non-toxicity, and has received a great deal of attention for its attractive optical properties and excellent stability. However, the existing double perovskite structure still has some defects, including lower electron dimension, larger band gap (generally more than 3 eV) and larger effective carrier mass.
Therefore, in order to solve the technical problems, the invention provides a nontoxic and stable layered double perovskite fluorescent material and a preparation method thereof.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a nontoxic and stable layered double perovskite fluorescent material and a preparation method thereof, wherein the fluorescent material can expand the application range of the existing non-layered double perovskite and provide a new thought for the photoelectric performance exploration of a double perovskite system.
In order to achieve the technical effects, the invention is realized by the following technical scheme: the layered double perovskite fluorescent material is characterized by being prepared from the following materials in percentage by mole:
CsX：50～60mol％；
MnX 2 ：10～20mol％；
BiX 3 ：20～30mol％；
wherein X is one or more of Cl, br, I, F elements.
Another object of the present invention is to provide a layered double perovskite fluorescent material and a preparation method thereof, which are characterized by comprising the steps of:
weighing CsX and MnX in proportion 2 、BiX 3 Mixing the raw materials, placing the mixed powder in an agate mortar, dripping deionized water or absolute ethyl alcohol, and grinding for 20-60 miAnd n, placing the ground massive powder into a drying oven at 90-100 ℃ for drying for 20-30 min, taking out, continuously grinding until the material is powdery, placing the ground mixture into a corundum crucible, then placing into a heating furnace for heating at a speed of 10 ℃/min, preserving heat for 1-5 h at 300-500 ℃, naturally cooling to room temperature, taking out the crucible, and grinding to obtain a powdery product, namely the layered double perovskite fluorescent material.
Further, the CsX and MnX 2 、BiX 3 The purity of the raw materials is 99.99 percent.
Further, the CsX and MnX 2 、BiX 3 The ratio of the mass of the raw materials to deionized water or absolute ethyl alcohol is 1 g/(4-7 ml).
Further, the heating furnace is a tube furnace or a box furnace.
Further, the atmosphere condition in the heating furnace is one or a combination of air, nitrogen and argon.
Compared with the prior art, the invention has the beneficial effects that:
the layered double perovskite of the invention has no toxicity compared with the traditional lead-based halide perovskite, and has good crystallinity and good stability to light, heat and humidity; the invention adopts a solid phase method, the raw materials are cheap and easy to obtain, no strong acid solvent polluting the environment is generated, no harmful waste is generated, the sample can be synthesized only at a lower reaction temperature, and the synthesized sample does not need further purification, thus the method is a simple, low-cost and environment-friendly synthesis method for synthesizing the layered double perovskite; the layered double perovskite disclosed by the invention can be matched with a commercial ultraviolet chip to emit orange-yellow light with the emission center near 600nm, and has a wide application prospect in the fields of illumination and display light and electricity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a Photoluminescence chart (PL) of a layered double perovskite fluorescent material according to an embodiment of the invention under excitation of a xenon lamp with a wavelength of 365nm as a light source at room temperature;
FIG. 2 is a graph of excitation spectrum (PLE) of a layered double perovskite fluorescent material according to an embodiment of the present invention under a condition that a monitored luminescence center is 601 nm;
FIG. 3 is a graphical X-ray diffraction (XRD) chart comparing ICSD#14996 with that of a layered double perovskite fluorescent material of an embodiment of the invention;
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of a layered double perovskite fluorescent material according to an embodiment of the present invention;
FIG. 5 is a graph of the energy spectrum (Energy dispersivespectroscopy, EDS) of a layered double perovskite fluorescent material according to an embodiment of the invention;
FIG. 6 is a Transmission Electron Microscope (TEM) diagram of a layered double perovskite fluorescent material according to an embodiment of the present invention and the interplanar spacings thereof;
FIG. 7 is a Thermogravimetric (TG) plot of a layered double perovskite fluorescent material according to an embodiment of the present invention;
fig. 8 is a photograph of an embodiment of a layered double perovskite fluorescent material of the present invention after a Light-emitting diode (LED) is packaged.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
An example layered double perovskite fluorescent material is prepared by weighing 57mol% of CsCl and 57mol% of MnCl according to the following proportion 2 14mol％、BiCl 3 28mol% of raw materials, mixing and then mixing the powderPlacing the powder into an agate mortar, dripping a proper amount of deionized water, grinding for 30min, placing the ground agglomerate powder into a 70 ℃ drying oven, drying for half an hour, taking out, continuously grinding until the material is powdery, transferring the material into a corundum crucible, placing into a muffle furnace at 450 ℃ for high-temperature sintering, sintering for 3h, and finally naturally cooling to room temperature to obtain the layered double perovskite fluorescent material.
Under the condition of room temperature, the photoluminescence spectrum (PL) of the fluorescent material is measured by using a Hitachi F-7000 fluorescence spectrophotometer, the xenon lamp light source is selected to be 365nm, and the result is shown in figure 1, and the photoluminescence spectrum of the layered double perovskite fluorescent material is broadband orange yellow light with the emission center at 601nm under the excitation of the 365nm xenon lamp.
Further by detecting 601nm wavelength, the excitation spectrum (PLE) of the phosphor can be measured, and the result is shown in FIG. 2, and three excitation peaks can be seen from the excitation spectrum, which correspond to Bi respectively 3+ Broadband ultraviolet characteristic excitation peak and Mn of (2) 2+ Characteristic excitation peaks at 430nm and 520 nm.
The layered double perovskite fluorescent material was tested by RigakuSmartLabSEX-ray diffraction (XRD) in Japan, and compared with the existing XRD in the ICSD database, and as a result, as shown in FIG. 3, the pure-phase layered double perovskite fluorescent material with good crystallinity can be obtained by the solid phase method.
The morphology of the phosphor was analyzed by a czech TESCANMIRALMS Scanning Electron Microscope (SEM), and the result is shown in fig. 4, and it can be seen that the synthesized layered double perovskite phosphor material exhibits a micrometer block shape with irregular size and shape. Fig. 5 shows the EDS spectrum of the layered double perovskite fluorescent material, with element distribution percentages matching the element content required for the actual synthesis, indicating that it can be successfully synthesized and that the synthesis process has good uniformity.
The microscopic morphology and lattice fringes of the phosphor were analyzed by a FEITalosf200S Transmission Electron Microscope (TEM) in the U.S. and the result is shown in FIG. 6, where the lattice fringe spacing was measured to be 0.294nm by digital micrograph software.
In order to further investigate the thermal stability of the layered double perovskite fluorescent material, the thermal gravimetric analysis of the fluorescent material was performed by TGA-4000, the heating time was 10 ℃/min, and the result is shown in fig. 7, and it can be seen that the layered double perovskite fluorescent material has no weight loss before 500 ℃, and shows good thermal stability.
Finally, in order to show the application of the fluorescent material in the illumination display field, the fluorescent material and a commercial ultraviolet LED chip are packaged (epoxy resin AB glue is used in the packaging process), and a luminous material diagram of the dried LED lamp bead through a miniature direct current power supply (2V, 0.2 MA) is shown as a figure 8, so that bright orange light emission is shown.
Example 2
Chinese patent (2022115724299) proposes: the rare earth doped multi-excitation light source optical temperature measurement type fluorescent powder is prepared from the following materials in percentage by mole: csX: 30-50 mol%; biX (BiX) 3 ：20～30mol％；ErX 3 :5 to 25mol%; x is one or more of Cl, br, I, F elements. The similarity between the components and the preparation method is higher, but the product properties and the application of the product are obviously different.
Rare earth doped multi-excitation light source optical temperature measurement type fluorescent powder, which is characterized in that Cs 3 Bi 2 Cl 9 By doping rare earth ions Er in a matrix which is a low-dimensional metal halide 3+ The optical temperature measurement type fluorescent powder excited by three near infrared lasers is classified as an up-conversion fluorescent material.
The substance synthesized by the invention is Cs 4 MnBi 2 Cl 12 The layered double perovskite material is a matrix material, is not doped, is first reported in 2020 and is synthesized by a hydrothermal method, is synthesized by a solid phase method for the first time, is cited as a luminescent lighting device, has been described by a characterization method and has been used for manufacturing an LED, and the excitation wavelength of the perovskite fluorescent powder is ultraviolet 365nm excitation, and belongs to a down-conversion luminescent material.
Secondly, the preparation process of the fluorescent material is basically similar, and the distinguishing characteristics are mainly characterized in that the temperature and time in each step are controlled, and the special temperature and time range can endow the material with special properties.
Again, erbium, element symbol Er, atomic number 68, is located in the periodic table of chemical elements at periodic 6, lanthanide (group IIIB) 11, atomic weight 167.26; manganese element symbol Mn, atomic number 25, in the fourth periodic zone of the periodic Table of the chemical elements, group VIIB; the two properties are far from each other and cannot be considered as conventional replacement means by those skilled in the art, and the former has no technical teaching on the latter.
Thus, the patent (2022115724299) does not affect the novelty and creativity of the present invention.
Claims (6)
1. The layered double perovskite fluorescent material is characterized by being prepared from the following materials in percentage by mole:
CsX：50～60mol％；
MnX 2 ：10～20mol％；
BiX 3 ：20～30mol％；
wherein X is one or more of Cl, br, I, F elements.
2. The preparation method of the layered double perovskite fluorescent material is characterized by comprising the following steps of:
weighing CsX and MnX in proportion 2 、BiX 3 Mixing the raw materials, placing the mixed powder in an agate mortar, dripping deionized water or absolute ethyl alcohol, grinding for 20-60 min, placing the ground slurry fluid into a drying oven at 90-100 ℃ for drying for 20-30 min, taking out, continuously grinding until the materials are powdery, placing the ground mixture into a corundum crucible, then placing the corundum crucible into a heating furnace for heating at a speed of 5 ℃/min, preserving heat for 1-5 h at 300-700 ℃, naturally cooling to room temperature, taking out the crucible, and grinding to obtain powdery products, namely the fluorescent powder material.
3. The method for preparing a layered double perovskite fluorescent material according to claim 2, wherein: the CsX and MnX 2 、BiX 3 The purity of the raw materials is equal99.99%.
4. The method for preparing a layered double perovskite fluorescent material according to claim 2, wherein: the CsX and MnX 2 、BiX 3 The ratio of the mass of the raw materials to deionized water or absolute ethyl alcohol is 1 g/(4-7 ml).
5. The method for preparing a layered double perovskite fluorescent material according to claim 2, wherein: the heating furnace is a tube furnace or a box furnace.
6. The method for preparing a layered double perovskite fluorescent material according to claim 2, wherein: the atmosphere condition in the heating furnace is one or a combination of air, nitrogen and argon.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116606653A (en) * | 2023-05-26 | 2023-08-18 | 昆明理工大学 | Preparation method of trivalent chromium ion doped broadband near infrared fluorescent material |
| CN116925766A (en) * | 2023-07-21 | 2023-10-24 | 昆明理工大学 | Yb (Yb) 3+ Preparation method of doped near infrared fluorescent material |
| CN116925767A (en) * | 2023-07-21 | 2023-10-24 | 昆明理工大学 | Er (Er) 3+ Method for preparing doped multimode and near infrared luminescent material |
| CN117089343A (en) * | 2023-08-25 | 2023-11-21 | 昆明理工大学 | Preparation method of near-infrared-light-emitting indium-based double perovskite |
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| CN110776914A (en) * | 2019-11-07 | 2020-02-11 | 中山大学 | Lead-free A 4MnBi 2X 12Preparation method and application of perovskite material |
| CN115084471A (en) * | 2022-07-01 | 2022-09-20 | 昆明理工大学 | Layered halide double perovskite lithium ion battery cathode material and preparation method thereof |
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| CN110776914A (en) * | 2019-11-07 | 2020-02-11 | 中山大学 | Lead-free A 4MnBi 2X 12Preparation method and application of perovskite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116606653A (en) * | 2023-05-26 | 2023-08-18 | 昆明理工大学 | Preparation method of trivalent chromium ion doped broadband near infrared fluorescent material |
| CN116925766A (en) * | 2023-07-21 | 2023-10-24 | 昆明理工大学 | Yb (Yb) 3+ Preparation method of doped near infrared fluorescent material |
| CN116925767A (en) * | 2023-07-21 | 2023-10-24 | 昆明理工大学 | Er (Er) 3+ Method for preparing doped multimode and near infrared luminescent material |
| CN117089343A (en) * | 2023-08-25 | 2023-11-21 | 昆明理工大学 | Preparation method of near-infrared-light-emitting indium-based double perovskite |
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